反应详情

To a stirred and cooled (ice bath, 10° C.) mixture of 3.4 parts of sodium tetrahydroborate and 188 parts of N,N-dimethylformamide were added dropwise 28 parts of (phenylmethyl) 4-(3-chloro-3-oxopropyl)-1-piperidinecarboxylate (exothermic reaction, the temperature rose to 38° C.). Upon completion addition, the reaction mixture was stirred over weekend at room temperature. The reaction mixture was poured into water and the product was extracted with methylbenzene. The extract was dried, filtered and evaporated, yielding 15.4 parts (61.6%) of (phenylmethyl) 4-(3-hydroxypropyl)-1-piperidinecarboxylate as a residue (int. 35).

1. temperaturecooled
2. customexothermic reaction
3. customrose to 38° C.
4. additionUpon completion addition
5. stirringthe reaction mixture was stirred over weekend at room temperature
6. extractionthe product was extracted with methylbenzene
7. customThe extract was dried
8. filtrationfiltered
9. customevaporated